CN104125987B - Manufacture height rich in cryptoxanthin and/or the method for the extract of its ester - Google Patents
Manufacture height rich in cryptoxanthin and/or the method for the extract of its ester Download PDFInfo
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Abstract
The invention provides a kind of manufacture containing cryptoxanthin and/or the method for the Fructus Lycii extract of its ester, said method comprising the steps of: a) obtain the Fructus Lycii being dried or its reduced size of fragment；And b) process above-mentioned dry Fructus Lycii or its reduced size of fragment with alkaline solution；And c) use solvent extraction in the middle Fructus Lycii being dried obtained of step b) or its reduced size of fragment, wherein said solvent is selected from ethyl acetate, hexane, heptane, petroleum ether, acetone, butane, methyl ethyl ketone, methanol, isopropanol and mixture thereof；And d) remove solvent from the extract obtained among step c)；And e) optionally, crack the ester in the dry extract obtained in step d)；And f) optionally, at acyclic straight or the C of side chain1‑4Alcohol crystallizes the dry extract obtained in step d) or step e).Preferably, only form to step f) by being given above step a) according to method of the present invention.
Description
Fructus Lycii (being commercially known as Fructus Lycii) is the logical of the fruit of two species the most closely-related
By name, described species are lycium barbarum (Lycium barbarum) and China Fructus Lycii (Lycium
Chinese), they are two species of Lycium (boxthorn).Due to Lycium barbarum
L. it is the species uniquely going through to use in China, therefore the invention particularly relates to Lycium barbarum
L. fruit-" Fructus Lycii ".
In all known food sources, the zeaxanthin of Fructus Lycii is the highest.Fructus Lycii in
The cultivation of state has decades, and it is used as food and uses in Traditional Chinese Medicine.In Fructus Lycii, class is recklessly
The content of Radix Raphani element is 600-900ppm.Main carotenoid is cryptoxanthin, described jade
Cream colour matter is presented in its natural esters.
The present inventor the most successfully develops a kind of lipophilic solvent extraction dried wolfberry
Method, and the oil of the oil rich in cryptoxanthin (content is 2-11 weight-%) is obtained with high yield
Property resin.This oleoresin can be further purified by crystallization from solvent (such as ethanol), from
And produce orange-red powder, wherein the content of zeaxanthin dipalmitate is 15-60 weight-%,
The content being equivalent to cryptoxanthin is 9-34 weight-%.Furthermore, it is possible to process containing cryptoxanthin two palm fibre
The oleoresin of palmitic acid acid esters is to crack this ester, thus the content producing cryptoxanthin is 30-95 weight %
Powder (productivity is 30-95%).
Therefore, the present invention relates to manufacture containing cryptoxanthin and/or the side of the Fructus Lycii extract of its ester
Method, said method comprising the steps of:
A) Fructus Lycii being dried or its reduced size of fragment are obtained；With
B) above-mentioned dry Fructus Lycii or its reduced size of fragment are processed with alkaline solution；With
C) Fructus Lycii being dried or its with solvent extraction acquisition in step b) are reduced size of broken
Sheet, wherein said solvent is selected from ethyl acetate, hexane, heptane, petroleum ether, acetone, butane, first
Methyl ethyl ketone methyl ketone, methanol, isopropanol and mixture thereof；With
D) solvent is removed from the extract obtained among step c)；With
E) optionally, the ester in the dry extract that cracking obtains in step d)；With
F) optionally, at acyclic straight or the C of side chain1-4Alcohol crystallizes in step d) or step e)
The dry extract of middle acquisition.
Any those skilled in the art should be understood that step e) and step f) is optional, because of
This is according in method of the present invention, they can be performed, it is also possible to be not carried out.Preferably
Ground, is only made up of to step f) step a) according to method of the present invention, and does not include any volume
Outer step.
According to the present invention one preferred embodiment relates to manufacturing containing cryptoxanthin (two) ester
The method of Fructus Lycii extract, said method comprising the steps of:
A) Fructus Lycii being dried or its reduced size of fragment are obtained；With
B) above-mentioned dry Fructus Lycii or its reduced size of fragment are processed with alkaline solution；With
C) Fructus Lycii being dried or its with solvent extraction acquisition in step b) are reduced size of broken
Sheet, wherein said solvent is selected from ethyl acetate, hexane, heptane, petroleum ether, acetone, butane, first
Methyl ethyl ketone methyl ketone, methanol, isopropanol and mixture thereof；With
D) solvent is removed from the extract obtained among step c)；With
F) optionally, at acyclic straight or the C of side chain1-4Alcohol crystallizes acquisition in step d)
Dry extract.
Another according to the present invention preferred embodiment relates to manufacturing the Fructus Lycii containing cryptoxanthin
The method of extract, described method comprises the steps of:
A) Fructus Lycii being dried or its reduced size of fragment are obtained；With
B) above-mentioned dry Fructus Lycii or its reduced size of fragment are processed with alkaline solution；With
C) Fructus Lycii being dried or its with solvent extraction acquisition in step b) are reduced size of broken
Sheet, wherein said solvent is selected from ethyl acetate, hexane, heptane, petroleum ether, acetone, butane, first
Methyl ethyl ketone methyl ketone, methanol, isopropanol and mixture thereof；With
D) solvent is removed from the extract obtained among step c)；With
E) ester in the dry extract that cracking obtains in step d)；With
F) optionally, in the C1-4 alcohol of acyclic straight or side chain, crystallize acquisition in step e)
Dry extract.
The method obtaining cryptoxanthin is known in the prior art, but it there are disadvantages that.
Such as, using aqueous extractant in CN-A 1 158 263, therefore contained in berry sugar is also
It is extracted out.
According to the method described in CN-A 1 086 730 focus on preserve Fructus Lycii natural nutrient component and
Flavour.
The method of US 2007/0161826 need use polar solvent (such as alcohol-water or acetone-water
Mixture) washing step (seeing [0021st] and [0024] section and the embodiment 3 of page 2).
The method of US 2005/0038271 is directed to use with oxolane and (was the most easily formed
Oxide) extraction step (seeing embodiment 2 and embodiment 3) or carry out in water crystallization step
Suddenly (seeing embodiment 4), wherein water is more straight than the aliphatic used in the step e) of the method for the present invention
Chain or the C of side chain1-4Alcohol wants difficulty to remove much.
Described in embodiment 3 according to WO 97/23436, first berry is put in water, removing sugar
After, it is dried the most again.
US 6,191,293 also describes with water pre-extracted China Fructus Lycii to remove the side of water-soluble gum
Method (sees embodiment 4).
The purpose of the method (seeing embodiment) of US 2008/0124416 is to obtain rich in polysaccharide and class Hu
The extract of Radix Raphani element, the extraction step therefore using water is necessary；But, the purpose of the present invention
To obtain height rich in the extract of cryptoxanthin, and the preferred form of described extract be powder and
Non-pastel, because the management of powder is much easier.
The method cost benefit that another advantage is that the present invention of the present invention is high, productivity high and can
Use at industrial scale to obtain a large amount of (several tons) natural cryptoxanthin and/or its ester
(especially its dipalmitate).
Now the method for the present invention is described in more detail.
Preferably, step f) is arrived all at noble gas ring according to the step a) of method of the present invention
Border (such as at nitrogen or argon or its mixture) performs.
Fructus Lycii can be lycium barbarum and/or China Fructus Lycii, preferably Lycium barbarum
L.。
Term " zeaxanthin ester " comprises cryptoxanthin monoesters and zeaxanthin diester.In Fructus Lycii
The zeaxanthin ester found is mainly two Palmic acid diester form of cryptoxanthin.
When only perform the step a) according to method of the present invention, b), c) and d) time, obtain
Be so-called " oleoresin ".Described oleoresin denseness at room temperature is starchy, its
Mainly it is made up of lipophilic compound (such as fat).In this oleoresin, with maize
It is (based on oleoresin total that the content of the cryptoxanthin presented in matter ester is usually 3-20 weight-%
Weight).
When only perform the step a) according to method of the present invention, b), c), d) and f) time,
Obtain be the content of cryptoxanthin (two) ester be 15-60 weight-% (gross weight based on extract
Amount) extract.This extract is powdery, and this makes to be very easy to its operation.
When perform according to the step a) of method of the present invention, b), c), d) and e) time, obtain
Be the content of cryptoxanthin (presented in free cryptoxanthin) be 30-95 weight-%
The extract of (gross weight based on extract).This extract is powdery, and this makes to operate it
Also it is very easy to.
Food supplement can be used as according to the extract that method of the present invention obtains, such as, be used for
Eye health.Additionally, described extract and the food supplement containing them can serve as antioxidant
And/or blue-light absorbers.
To retouch in more detail according to the single step of method of the present invention below now
State.
Step a): obtain the Fructus Lycii or its reduced size of fragment being dried
The Fructus Lycii being dried generally can be commercially available.The Fructus Lycii being dried being commercially available
It is used directly for the present invention.
It is optionally possible to reduce the size of the Fructus Lycii being dried.If it has been found that reduced before extraction
The size of the Fructus Lycii being dried, then the extract extracted in step c) (as mentioned below)
The concentration of middle cryptoxanthin can be higher.
Any method well known by persons skilled in the art can be used to complete the reduction of size.Preferably side
Method is that machinery reduces, such as, crush, pulverize, shred and grind, wherein crush and grind and combinations thereof
It is preferred.
The preferred embodiment of the present invention is also some preferred implementations of step a) listed above
Combined embodiment.
Step b): process with alkaline solution
In step b), process with alkaline solution the Fructus Lycii being dried obtained in the step a) or its
Reduced size of fragment.
The alkaline solution used in step b) can be that the alkalescence of any pH ＜ 12 known in the art is molten
Liquid.The example of this kind of alkaline solution is including, but not limited to Na2CO3、K2CO3、Ca(OH)2、
NaHCO3And KHCO3Aqueous solution, ammonia and NH3Deng.According to preferred alkali of the present invention
Property solution is Na2CO3The Na of aqueous solution, such as 0.3mol/L-0.5mol/L2CO3Aqueous solution.
The amount of the alkaline solution that can add is 1-5 liter, preferably 1-4 liter, more preferably 1-3 liter,
It is even furthermore preferable that 1.5-2.5 liter, most preferably 2 liters, wherein said amount is to exist relative to every 1kg
The Fructus Lycii being dried obtained in step a) or the amount of its reduced size of fragment.
Described process is executed once or repeatedly, such as 1 time, 2 times or 3 times.Process sustainable every time
At least 10 minutes, preferably 20 minutes-1 hour, most preferably 30 minutes.
After process, can add in the mixture containing the Fructus Lycii being dried or its reduced size of fragment
Acid is to neutralize.This neutralization is not necessary to carry out, and therefore according to the present invention, it can be performed, also
Can be not carried out.However it has been found that is added adds in step c) for the acid neutralized
(as mentioned below) content of cryptoxanthin and productivity in the extract obtained in.This area any
Technical staff can understand, any acid known in the art can be used in this purpose.In this step
The acid being preferably used is mineral acid, such as HCl.Preferably, containing the Fructus Lycii being dried or its size
It is 7-8 that the mixture of the fragment reduced is neutralized to pH, and preferred pH is 7.5.
After process, Fructus Lycii or its reduced size of fragment can be leached from mixture, then by it
Directly or after drying it is used for next step.
Preferably, step b) performs at 10 DEG C-30 DEG C, more preferably performs at 15 DEG C-25 DEG C,
The most at room temperature perform.
Have been found that step b) can remove the by-product in Fructus Lycii or its reduced size of fragment more than 70%
Product, therefore can extracted residues, Er Qiesuo easily in step c) (as mentioned below)
State process extraction efficiency to be made to double and make the solvent used in step c) reduce 70%.
Step c): extraction
In step c), extract the Fructus Lycii or its reduced size of fragment obtained in step b).
Extraction in step c) can be performed a number of times, preferably 3 times.It is of course also possible to only carry out
1 time or 2 described extractions, but extraction time is longer.
Extraction continues 30 minutes-2 hours the most every time, preferably 45 minutes-1 hour.This area
Technical staff can find out the most efficient time needed for extraction easily.
Preferably, the extractant used in the step c) be the volume ratio of ethyl acetate and hexane be 1:
The mixture of 1, single ethyl acetate and single hexane.Most preferably extractant is acetic acid second
Ester.
Preferably, the amount of the solvent used in step c) is 0.3-2 liter, more preferably 0.3-1.2
Rising, it is even furthermore preferable that 0.3-0.6 liter, wherein said amount is to obtain in step a) relative to every 1kg
The Fructus Lycii being dried obtained or the amount of its reduced size of fragment.
Preferably, step c) performs at 20 DEG C-80 DEG C, more preferably performs at 30 DEG C-70 DEG C,
Even more preferably still perform at 40 DEG C-70 DEG C, most preferably perform at 50 DEG C-65 DEG C.
If the extract obtained in step c) contains insoluble part, preferably will by filtration
It removes.
The preferred embodiment of the present invention is also some preferred implementations of step c) listed above
Combined embodiment.
Step d): remove solvent
In step d), the solvent in the extract obtained in step c) is removed to obtain " oil
Property resin ".
Can remove molten from the extract obtained among step c) by any method known in the art
Agent, such as by being evaporated under reduced pressure.
Preferably, remove solvent and perform at 20 DEG C-78 DEG C, more preferably hold at 30 DEG C-50 DEG C
OK, most preferably perform at 40 DEG C-45 DEG C.
Solvent can be removed in batches, in a serial fashion or in a continuous manner.
The preferred embodiment of the present invention is also some preferred implementations of step d) listed above
Combined embodiment.
Step e): cracking ester
Being present in the cryptoxanthin in the oleoresin obtained in step d) is esterification mostly, and
Main presented in zeaxanthin dipalmitate.In order to obtain free cryptoxanthin, it is necessary to
Oleoresin is processed to crack ester with alkali (such as KOH and/or NaOH).If processed with aqueous alkali,
Cryptoxanthin and soap (saponification) will be obtained simultaneously.If at acyclic straight or the C of side chain1- 4Alcohol processes with alkali (such as with solid KOH and/or solid NaOH), cryptoxanthin will be obtained simultaneously
With fatty acid ester (ester exchange).
Optionally, the oleoresin obtained in the step d) can experience the process of saponification or ester exchange with
Obtain free cryptoxanthin.
Preferably, the cracking of zeaxanthin ester is completed by ester exchange.It is highly preferred that ester exchange exists
Perform at 20 DEG C-120 DEG C, preferably perform at 60 DEG C-100 DEG C, more preferably at 70 DEG C-90 DEG C
Perform.Can complete described reaction under ambient pressure or higher pressure, this depends on selected
Temperature.
Most preferably, ester exchange is by the presence of alkali, zeaxanthin ester and acyclic straight or
The C of chain1-4The reaction of alcohol completes.
Acyclic straight or the C of side chain1-4The example of alcohol be methanol, ethanol, isopropanol, normal propyl alcohol,
N-butyl alcohol, isobutanol and the tert-butyl alcohol.Preferably alcohol is methanol and ethanol and arbitrary mixture thereof.?
Preferably alcohol is ethanol.
Preferably, the amount of described alcohol is 2-12 liter (extract being dried relative to every kg), more preferably
Be 4-10 liter (extract being dried relative to every kg), most preferably 5-8 liter is (relative to every kg
The oleoresin obtained in step d)).
The example of alkali is alkali metal hydroxide, such as KOH and NaOH and arbitrary mixture thereof.
Preferably, the amount of described alkali is at stoichiometry (stoichiometrical amount) or catalytic amount
In the range of, such as 25-40 weight-%'s (oleoresin based on obtaining in step d))
KOH。
The preferred embodiment of the present invention is also some preferred implementations of step e) listed above
Combined embodiment.
Step f): crystallization
Optionally, in step f), can be at acyclic straight or the C of side chain1-4Alcohol crystallizes in step
Rapid oleoresin d) or obtained in step e) is to concentrate cryptoxanthin or its ester.
If step e) is completed by ester exchange, then the aliphatic used in step f) is straight
Chain or the C of side chain1-4Alcohol is identical with use in step e).The alcohol being preferably used in step e)
It is equally applicable to herein.Therefore, in step f), solvent most preferably with is ethanol.
When crystallizing in ethanol, step f) preferably performs at room temperature-78 DEG C, more preferably
Ground performs at 40 DEG C-60 DEG C, most preferably performs at about 50 DEG C.
When being not carried out step e), the amount preferably 1-10 liter of the alcohol used in step f),
More preferably 2-7 liter, most preferably 3-5 liter, wherein said amount is in step relative to every 1kg
The amount of the oleoresin obtained in d).
The preferred embodiment of the present invention is also some preferred implementation phases of step f) listed above
The embodiment of combination.
The preferred embodiment of the present invention is step a) listed above and/or step b) and/or step
Rapid c) and/or the one or more preferred embodiment party of step d) and/or step e) and/or step f)
The embodiment that formula is combined.
Very particularly preferred embodiment of the invention is to manufacture the side of the Fructus Lycii extract containing cryptoxanthin
Method, said method comprising the steps of:
A) Fructus Lycii being dried or its reduced size of fragment are obtained；With
B) Na is used2CO3Solution processes above-mentioned dry Fructus Lycii or its reduced size of fragment；With
C) at 40 DEG C-50 DEG C, it is extracted with ethyl acetate the Fructus Lycii being dried obtained in step b)
Son or its reduced size of fragment；With
D) solvent is removed from the extract obtained among step c)；With
F) in the presence of alkali, the dry extraction obtained in step d) by ester exchange cracking with ethanol
Ester in thing.
Another most preferred embodiment of the present invention is to manufacture the Chinese holly containing cryptoxanthin (two) ester
The method of Fructus Lycii extract, said method comprising the steps of:
A) Fructus Lycii being dried or its reduced size of fragment are obtained；With
B) Na is used2CO3Solution processes above-mentioned dry Fructus Lycii or its reduced size of fragment；With
C) at 40 DEG C-50 DEG C, it is extracted with ethyl acetate the Fructus Lycii being dried obtained in step b)
Son or its reduced size of fragment；With
D) solvent is removed from the extract obtained among step c)；With
E) dry extract obtained in step d) is crystallized in ethanol.
To be further elucidated with the present invention by following non-limiting embodiment now.
Embodiment
For the purpose analyzed, it is thus achieved that the sample of all products be all saponified, the most contained therein
Zeaxanthin ester is measured with the form of free cryptoxanthin.So, cryptoxanthin given below
Content always refer to the cryptoxanthin of cryptoxanthin rather than the esterification dissociated.
Even if the most clearly mentioning, all of embodiment all performs in inert gas environment.
Embodiment 1: by with Na
2
CO
3
/ HCl processes and is extracted with ethyl acetate and manufactures oleoresin
The Fructus Lycii being dried is purchased from Zhaokang Fructus Lycii company limited (Zhaokang Goiiberry
Inc., central arid belt in Ningxia, China).Pulverize 100.28g Fructus Lycii and use 100mL Na2CO3
(0.3mol/L) pretreatment, is stirred at room temperature 30min, then with 1mol/L HCl regulation pH extremely
7.5.Process said mixture 3 times by 200mL ethyl acetate, at 50 DEG C, stir 1h.Then obtain
1.8861g oleoresin.Wherein the content of cryptoxanthin is 5.11%, and productivity is 90.50%.Productivity meter
Calculation formula is: productivity=((product assay × products weight)/(oleoresin content × oleoresin
Weight)) × 100
Embodiment 2: by with Na
2
CO
3
/H
2
O processes and manufactures oleoresin with hexane extraction
The Fructus Lycii being dried is purchased from Zhaokang Fructus Lycii company limited (central arid belt in Ningxia, China).
The Fructus Lycii powder being dried by 101.1g is put in the flask of 500mL.Add 200mL 0.3M Na2CO3
And it is stirred at room temperature 30min.Under 1.5bars, leach solid with pressure filter, then exist
With 200mL ethyl acetate stirring extraction 45min at 45 DEG C.Repeat to extract 3 times, be then combined with extraction
Thing.Add 20g Na2SO4To slough the water in extract, continue 1h, then leach Na2SO4.?
After vacuum using Rotary Evaporators remove the solvent in extract, obtain the wine-colored oiliness of 1.2681g
Resin.Wherein the productivity of cryptoxanthin is 39.98%, and content is 2.19%.Calculation of yield formula is:
Productivity=((product assay × products weight)/(oleoresin content × oleoresin weight)) ×
100
Embodiment 3: by manufacturing oleoresin with less than the ethyl acetate extraction in embodiment 1
The Fructus Lycii being dried is purchased from Zhaokang Fructus Lycii company limited (central arid belt in Ningxia, China).
The Fructus Lycii powder being dried by 100.6g is put in the flask of 500mL.Add 200mL 0.3M Na2CO3
And it is stirred at room temperature 30min.In flask, add 1M HCl carefully and keep rocking, until mixed
The pH of compound is adjusted to 7.5.Under 1.5bars, leach solid with pressure filter, then exist
With 100mL ethyl acetate stirring extraction 45min at 45 DEG C.Repeat to extract 3 times, be then combined with extraction
Thing.Add 20g Na2SO4To slough the water in extract, continue 1h, then leach Na2SO4.?
After vacuum using Rotary Evaporators remove the solvent in extract, obtain the wine-colored oiliness of 0.9365g
Resin.Wherein the productivity of cryptoxanthin is 77.51%, and content is 5.72%.Calculation of yield formula is:
Productivity=((product assay × products weight)/(oleoresin content × oleoresin weight)) ×
100
Embodiment 4: yellow to manufacture rich in natural corn by crystallizing purification oleoresin in ethanol
The powder of matter
By the oleoresin (content of cryptoxanthin is 51.1g/kg) in 1.65g embodiment 1 point to 8ml
In ethanol.At 50 DEG C, stir said mixture 30min, be then cooled to room temperature and keep 2h.Filter
Go out the solid formed, with cool washing with alcohol (4 DEG C, 5ml, 3 times) and in fine vacuum dry.Obtain
Obtained 211.7mg product.Being analyzed by HPLC, the content of cryptoxanthin is 307.4g/Kg, productivity
It is 77.18%.Calculation of yield formula is: productivity=((product assay × products weight)/(oiliness tree
Fat content × oleoresin weight)) × 100
Embodiment 5: the ester exchange carrying out zeaxanthin ester in oleoresin is brilliant with release cryptoxanthin
Body
Oleoresin in 2.43g embodiment 1 and 29ml ethanol are mixed and heated to (the 130 DEG C of oil that reflux
Bath), in 5min, then add the ethanol solution of 20ml KOH (0.32g) the 20min that refluxes.With
After, remove oil bath pan, in 10min, be added dropwise over 0.8ml acetic acid, then allow mixture to be cooled to
Room temperature also keeps 3h.With ethanol (20ml), the ethanol of 1: 1: water (20ml), water (40ml)
Wash, with ethanol (20ml), the solid formed and be dried in a vacuum.Obtain 53.5mg product.Wherein
The content of free cryptoxanthin is 182.6 g/Kg, and productivity is 13.14%.
Claims (28)
1. manufacturing containing cryptoxanthin and/or the method for the Fructus Lycii extract of its ester, described method includes
Following steps:
A) Fructus Lycii being dried or its reduced size of fragment are obtained；With
B) above-mentioned dry Fructus Lycii or its reduced size of fragment are processed with alkaline solution；With
C) Fructus Lycii being dried obtained in step b) with solvent extraction or its reduced size of fragment,
Wherein said solvent is selected from ethyl acetate, hexane, heptane, petroleum ether, acetone, butane, methyl second
Base ketone, methanol, isopropanol and mixture thereof, and wherein obtain in step a) relative to every 1kg
Be dried Fructus Lycii or the amount of its reduced size of fragment, the amount of the solvent of use is 0.3-2 liter；With
D) solvent is removed from the extract obtained among step c)；With
E) optionally, the ester in the dry extract that cracking obtains in step d)；With
F) optionally, at acyclic straight or the C of side chain1-4Alcohol crystallizes in step d) or step e)
The dry extract of middle acquisition.
Method the most according to claim 1, wherein said method only by step a) to step f) group
Become and do not include any extra step.
Method the most according to claim 1, wherein the size in step a) reduces is to pass through
Machinery has reduced.
Method the most according to claim 1, the pH of the alkaline solution wherein used in step b)
＜ 12.
Method the most according to claim 4, the alkaline solution wherein used in step b) is selected from:
Na2CO3、K2CO3、Ca(OH)2、NaHCO3And KHCO3Aqueous solution, ammonia and NH3。
Method the most according to claim 5, the alkaline solution wherein used in step b) is
The Na of 0.3mol/L-0.5mol/L2CO3Solution.
Method the most according to claim 1, the amount of the alkaline solution wherein used in step b)
Being 1-5 liter, wherein said amount is the Fructus Lycii being dried or its obtained in step a) relative to every 1kg
The amount of reduced size of fragment.
Method the most according to claim 1, the amount of the alkaline solution wherein used in step b)
Being 1.5-2.5 liter, wherein said amount is the Fructus Lycii being dried obtained in step a) relative to every 1kg
Or the amount of its reduced size of fragment.
9., according to the method described in claim 1-5 any one, wherein step b) is additionally included in and uses alkali
Property solution process after, neutralize with acid.
Method the most according to claim 9, wherein said acid is mineral acid.
11. methods according to claim 9, wherein said acid is mineral acid HCl.
12. methods according to claim 9, the Fructus Lycii being dried wherein processed by alkaline solution
It is 7-8 that son or its reduced size of fragment are neutralized to pH.
13. according to the method described in claim 1-5 any one, and wherein step b) is at 10 DEG C-30 DEG C
Lower execution.
14. according in the method described in claim 1-5 any one, and wherein step b) at room temperature holds
OK.
15. methods according to claim 1, wherein step c) is performed 3 times.
16. methods according to claim 1, the solvent wherein used in step c) is acetic acid second
The volume ratio of ester and hexane is the mixture of 1:1.
17. methods according to claim 1, the solvent wherein used in step c) is acetic acid second
Ester.
18. methods according to claim 1, the solvent wherein used in step c) is hexane.
19. methods according to claim 1, the amount of the solvent wherein used in step c) is
0.3-0.6 liter, wherein said amount be the Fructus Lycii being dried obtained in the step a) relative to every 1kg or
The amount of its reduced size of fragment.
20. methods according to claim 1, wherein step c) performs at 20 DEG C-80 DEG C.
21. methods according to claim 1, the acyclic straight wherein used in the step f) or
The C of side chain1-4Alcohol is ethanol.
22. methods according to claim 1, wherein step f) performs at room temperature to 78 DEG C.
23. methods according to claim 21, do not perform step d) and in step f)
The amount of the ethanol used is 1-10 liter, and wherein said amount obtains in step d) relative to every 1kg
The amount of oleoresin.
24. methods according to claim 1, wherein in step e), the cracking of zeaxanthin ester is logical
Cross the saponification of the zeaxanthin ester in the dry extract obtained in step d) or ester exchange completes.
25. methods according to claim 1, wherein the cracking of zeaxanthin ester is to pass through ester exchange
Ester exchange in that complete and step e) performs at 20 DEG C-120 DEG C.
26. methods according to claim 25, wherein ester exchange is by the presence of alkali, Semen Maydis
Xanthin ester and acyclic straight or the C of side chain1-4Alcohol carries out having reacted.
27. methods according to claim 26, the extraction that the amount of wherein said alcohol is dried relative to every kg
Taking thing is 2-12 liter.
28. according to the method described in claim 26 or 27, and the amount of wherein said alkali is at catalytic amount extremely chemistry
In the range of metered amount.
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| PCT/CN2013/000176 WO2013127255A1 (en) | 2012-02-27 | 2013-02-22 | Process for manufacture of highly enriched extract containing zeaxanthin and/or its esters |
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| US5648564A (en) * | 1995-12-21 | 1997-07-15 | Kemin Industries, Inc. | Process for the formation, isolation and purification of comestible xanthophyll crystals from plants |
| US6191293B1 (en) * | 1998-04-20 | 2001-02-20 | Inexa, Industria Extractora C.A. | Trans-xanthophyll ester concentrates of enhanced purity and methods of making same |
| WO2003048284A1 (en) * | 2001-11-29 | 2003-06-12 | University Of Maryland | Process for extraction and purification of lutein, zeaxanthin and rare carotenoids from marigold flowers and plants |
| CN1578628A (en) * | 2001-09-04 | 2005-02-09 | 利库德天然产品工业有限公司 | Carotenoid extraction process |
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| US5648564A (en) * | 1995-12-21 | 1997-07-15 | Kemin Industries, Inc. | Process for the formation, isolation and purification of comestible xanthophyll crystals from plants |
| US6191293B1 (en) * | 1998-04-20 | 2001-02-20 | Inexa, Industria Extractora C.A. | Trans-xanthophyll ester concentrates of enhanced purity and methods of making same |
| CN1578628A (en) * | 2001-09-04 | 2005-02-09 | 利库德天然产品工业有限公司 | Carotenoid extraction process |
| WO2003048284A1 (en) * | 2001-11-29 | 2003-06-12 | University Of Maryland | Process for extraction and purification of lutein, zeaxanthin and rare carotenoids from marigold flowers and plants |
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